EP0691539A2 - Verfahren zur Herstellung von amperometrischen Elektroden - Google Patents

Verfahren zur Herstellung von amperometrischen Elektroden Download PDF

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Publication number
EP0691539A2
EP0691539A2 EP95109199A EP95109199A EP0691539A2 EP 0691539 A2 EP0691539 A2 EP 0691539A2 EP 95109199 A EP95109199 A EP 95109199A EP 95109199 A EP95109199 A EP 95109199A EP 0691539 A2 EP0691539 A2 EP 0691539A2
Authority
EP
European Patent Office
Prior art keywords
electrode
making
amperometric
recited
applying
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP95109199A
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English (en)
French (fr)
Other versions
EP0691539B1 (de
EP0691539A3 (de
Inventor
Larry D. Johnson
Alison J. Murray
Matthew K. Musho
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Bayer Corp
Original Assignee
Bayer AG
Bayer Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Bayer AG, Bayer Corp filed Critical Bayer AG
Publication of EP0691539A2 publication Critical patent/EP0691539A2/de
Publication of EP0691539A3 publication Critical patent/EP0691539A3/de
Application granted granted Critical
Publication of EP0691539B1 publication Critical patent/EP0691539B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/28—Electrolytic cell components
    • G01N27/30—Electrodes, e.g. test electrodes; Half-cells
    • G01N27/327—Biochemical electrodes, e.g. electrical or mechanical details for in vitro measurements
    • G01N27/3271—Amperometric enzyme electrodes for analytes in body fluids, e.g. glucose in blood
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S435/00—Chemistry: molecular biology and microbiology
    • Y10S435/817—Enzyme or microbe electrode

Definitions

  • the present invention generally relates to biosensors, and, more particularly, to new and improved amperometric electrodes and a method of making the amperometric electrodes.
  • Amperometric electrodes or biosensors, such as a glucose biosensor, are used for electrochemical measurements.
  • a sample is applied to the amperometric electrodes, and a resulting current is measured for a test sample.
  • the resulting current should have sufficient magnitude to facilitate measurement and have reproducibility to provide a meaningful test result.
  • amperometric electrodes Time consuming and undesirable processes, such as polishing and heat treatment, have been required for known amperometric electrodes to achieve the required current response.
  • Important objects of the present invention are to provide a new and improved method of making and amperometric electrode; to provide amperometric electrodes that provide reliable, reproducible and effective operation and to provide amperometric electrodes for a blood glucose biosensor.
  • the objects and advantages of the present invention are achieved by a method of making and an amperometric electrode.
  • An electrode carbon ink is applied to a polymer substrate to form a working electrode.
  • the substrate carrying the working electrode is placed in a gas plasma cleaner, such as an oxygen or nitrogen plasma, to clean the working electrode.
  • a high radio frequency signal excites the gas plasma for a short exposure time in a range between 10 seconds and 30 seconds.
  • a reagent layer is deposited to the plasma-treated working electrode.
  • Amperometric electrodes 12 include an end portion 12A for receiving a test sample and an opposite end lead/contact pad portion 12B for connection with an instrument 14 capable of imposing a voltage potential and measuring the resulting current.
  • the amperometric electrodes 12 include a working electrode 16 formed by an electrode carbon ink, for example, by screen printing onto a polymer substrate 18 and then thermally drying. A reagent layer 20 is deposited over the working electrode 16 after the working electrodes have been plasma treated in accordance with the present invention.
  • thermoplastic material such as a polycarbonate or polystyrene, having sufficient physical and electrical insulating properties can be used for the polymer substrate 18.
  • the electrode carbon ink forming the working electrodes 16 can contain 18% graphite and 6% carbon black.
  • the working electrodes 16 can be formed with an Acheson 423ss ink screen printed onto a polystyrene substrate 18.
  • sensor cards 10 with carbon working electrodes 16 are thermally dried and then placed into a chamber 22 of a plasma cleaner 24.
  • a small barrel plasma etcher sold by March Instruments can be used for the plasma cleaner 24.
  • the chamber 22 is first evacuated to 0.1-0.2 Torr and then backfilled with a gas, such as oxygen (O2) or nitrogen (N2), to an operating pressure of 0.3-0.5 Torr. Once the pressure stabilizes, the gas is excited by a radio frequency (RF) signal source 26 having a frequency of 13.56 Mhz and a power level typically of 20-25 watts.
  • RF radio frequency
  • the sensor cards 10 are removed from the chamber 22 and are ready for chemistry deposition or testing. Then the reagent layer 20 containing an enzyme, such as glucose oxidase for a blood glucose biosensor, and a mediator or electron transfer agent is deposited over the treated surface of the working electrode 16.
  • an enzyme such as glucose oxidase for a blood glucose biosensor
  • a mediator or electron transfer agent is deposited over the treated surface of the working electrode 16.
  • Photomicrographs of the carbon working electrodes 16 before and after the gas plasma treatment do not show any observable physical change. However, the current response of the untreated and treated carbon working electrodes 16 are significantly different. Erratic behavior with little or no current is replaced by high, reproducible currents for the gas plasma treated electrodes 16.
  • Polymeric binders such as polyvinyl chloride that are deposited with the carbon during screen printing of the working electrodes 16 are believed to be the primary material removed during the gas plasma cleaning treatment.
  • FIG. 4 illustrates the effect of plasma treatment time on the performance of the amperometric electrodes 16.
  • Treatment time is shown in seconds along the horizontal axis with a resulting current for the test solution in micro-amperes ⁇ A shown along the vertical axis.
  • sensors were constructed by screen printing two carbon electrodes 16 using Acheson 423ss ink onto a polystyrene substrate 18. Two other printings were provided; one for the leads/contact pads 12B and another for an overcoat dielectric layer which protects the leads/contact pads 12B from the test solution.
  • a selected plasma treatment time was provided, as illustrated in FIG. 4.
  • FIG. 5 the same protocol as described with respect to FIG. 4 was used, except that the testing solution concentration was varied over the range of 0 to 30 mM potassium ferrocyanide.
  • the testing solution concentration is shown along the horizontal axis with a resulting current for the test solution in microamperes ⁇ A shown along the vertical axis.
  • Two plasma-cleaning times of 10 seconds and 20 seconds are illustrated by a line labelled 10S and a line labelled 20S, respectively.
  • the resulting current corresponds to the reduced mediator of the reagent layer 20.
  • the reagent layer is based on an aqueous polymer solution containing the required reagents for a particular biosensor.
  • Electrodes are constructed using conductive and dielectric inks printed on a 3" x 3" polycarbonate substrate.
  • Conductive ink used for the active areas is Acheson 421ss which is screen printed on and then thermally cured.
  • the areas of the electrodes are defined by an overcoat of dielectric (Acheson 452ss) which is screen printed on and then UV cured.
  • Activating the printed electrodes requires treating cards in a plasma etcher. In our case we used either a small barrel-cavity instrument from March Instruments or a tray instrument from Branson/IPC. Cards are loaded on the shelves of a Branson/IPC plasma etcher.
  • the plasma treater is evacuated to 0.1-0.2 torr, then backfilled with purified oxygen gas to a pressure of .8 torr. After a plasma is generated, the cards are treated for three minutes at 300 watts of power. Testing the activated electrodes requires that each sensor's leads be connected to a potentiostat for testing. This can be done in the card format or as singulated electrodes.
  • the electrodes themselves are dipped into a solution containing 200 mM potassium Ferricyanide, 12.5 mM Potassium Ferrocyanide and 100 mM phosphate buffer pH 7. A positive 400 millivolts are applied across the working and reference electrodes, and the current is measured at the working electrode.

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  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • Hematology (AREA)
  • General Physics & Mathematics (AREA)
  • Molecular Biology (AREA)
  • Pathology (AREA)
  • Measuring Or Testing Involving Enzymes Or Micro-Organisms (AREA)
  • Investigating Or Analysing Biological Materials (AREA)
  • Surface Acoustic Wave Elements And Circuit Networks Thereof (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Electrical Discharge Machining, Electrochemical Machining, And Combined Machining (AREA)
  • Electrodes Of Semiconductors (AREA)
EP95109199A 1994-06-27 1995-06-14 Verfahren zur Herstellung von amperometrischen Elektroden Expired - Lifetime EP0691539B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US08/265,913 US5429735A (en) 1994-06-27 1994-06-27 Method of making and amperometric electrodes
US265913 1994-06-27

Publications (3)

Publication Number Publication Date
EP0691539A2 true EP0691539A2 (de) 1996-01-10
EP0691539A3 EP0691539A3 (de) 1996-07-24
EP0691539B1 EP0691539B1 (de) 2006-12-13

Family

ID=23012394

Family Applications (1)

Application Number Title Priority Date Filing Date
EP95109199A Expired - Lifetime EP0691539B1 (de) 1994-06-27 1995-06-14 Verfahren zur Herstellung von amperometrischen Elektroden

Country Status (10)

Country Link
US (1) US5429735A (de)
EP (1) EP0691539B1 (de)
JP (1) JP3513260B2 (de)
AT (1) ATE348333T1 (de)
AU (1) AU692861B2 (de)
CA (1) CA2151413C (de)
DE (1) DE69535334T2 (de)
DK (1) DK0691539T3 (de)
ES (1) ES2277331T3 (de)
PT (1) PT691539E (de)

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PT691539E (pt) 2007-03-30
JP3513260B2 (ja) 2004-03-31
AU692861B2 (en) 1998-06-18
AU2325795A (en) 1996-01-11
EP0691539B1 (de) 2006-12-13
US5429735A (en) 1995-07-04
CA2151413A1 (en) 1995-12-28
JPH0815210A (ja) 1996-01-19
ATE348333T1 (de) 2007-01-15
DE69535334T2 (de) 2007-05-31
DK0691539T3 (da) 2007-04-02
EP0691539A3 (de) 1996-07-24
CA2151413C (en) 2004-08-24
DE69535334D1 (de) 2007-01-25
ES2277331T3 (es) 2007-07-01

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